CN102092828A - Method for preparing polymer calcium-aluminum silicate coagulant from carbide slag - Google Patents
Method for preparing polymer calcium-aluminum silicate coagulant from carbide slag Download PDFInfo
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- CN102092828A CN102092828A CN 201010583622 CN201010583622A CN102092828A CN 102092828 A CN102092828 A CN 102092828A CN 201010583622 CN201010583622 CN 201010583622 CN 201010583622 A CN201010583622 A CN 201010583622A CN 102092828 A CN102092828 A CN 102092828A
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Abstract
The invention discloses a method for preparing an agent for treating water, wastewater and sewage, particularly the method for preparing a polymer calcium-aluminum silicate coagulant from carbide slag, which is characterized by comprising the following steps of: drying the carbide slag; purifying the dried carbide slag by using ammonium chloride to obtain carbide slag extract; preparing solution of sodium silicate, and adjusting a pH value of the solution of sodium silicate by using a concentrated sulfuric acid or sodium hydroxide to obtain polymer silicate solution; performing condensation polymerization on the polymer silicate solution to obtain high polymer silicate solution; and performing sedimentation on the high polymer silicate solution, solution of aluminum sulfate and the carbide slag to prepare the polymer calcium-aluminum silicate coagulant product. The method has the advantages of scientificity, rationalism, low energy consumption, low cost and the like; and the polymer calcium-aluminum silicate coagulant prepared by the method has high stability and ensures good water treatment effects.
Description
Technical field
The present invention is the preparation method of a water, waste water, sewage-treating agent, is a kind of method of utilizing carbide slag to prepare calcium polysilicate aluminium coagulating agent.
Background technology
Polysilicate class coagulating agent is a kind of inorganic polymer coagulant.At present, the method for developing polysilicate coagulant both at home and abroad mainly is divided into three kinds: the one, and the poly-silicic acid flocculation agent of metal ion, the 2nd, recombining process gathers the silicic acid compound coagulant, and the 3rd, copolymerization process gathers the silicic acid flocculation agent.Poly-silicic acid and metal-salt directly mix the poly-silicic acid flocculation agent that the poly-silicic acid metal composite coagulating agent of generation belongs to metal ion; To gather silicic acid and polymer/metallic salt, to be mixed and made into the PASM flocculation agent be the poly-silicic acid of recombining process; Mixing earlier the back with metallic salt is copolymerization process at the flocculation agent that adding OH makes its polymerization.In addition, doing raw material with ore, abandoned mine slag, flyash etc. develops novel coagulating agent and has had related.
" safety and environment journal " 2002 1 phases 2 volume, the carbide slag and the CaCl of people's experimental studies such as Li Yafeng
2To the coagulating treatment effect of Shenyang Tiefa Mine Administration black water and adopt carbide slag-PAM coagulant sedimentation to handle the back black water, every index all can reach the report of discharging standards.Open (bulletin) number CN1778702 of Chinese invention patent discloses people such as Zhao Qinghai invention, name is called " a kind of sewage-treating agent and its production and application ", this sewage-treating agent is made up of coagulating agent and coagulant aids two portions, composite use, coagulant aids is made by the raw material of following weight part: carbide slag 8～20, preparation water 600～1000.Use treatment agent of the present invention to handle town sewage or industrial sewage, can reach the purpose of purification of water quality.
There are weak point in traditional low molecule, polyphosphazene polymer silicic acid composite coagulant at aspects such as molecular conformation, the polymerization degree and corresponding flocculation-flocculating results more, therefore, be necessary development of new efficiently compound coagulant compensate its defect.To gather silicic acid and inorganic metal salt coagulant double crossing, the novel inorganic polymer polysilicate coagulant that processability is stable.The present invention brings into play the advantage of poly-silicic acid, remedies the shortcoming of metal-salt self, produces synergy.Be that raw material and high polysilicate prepare coagulating agent and be applied to water treatment field and do not appear in the newspapers as yet with the carbide slag.
Content of the present invention
The objective of the invention is, prior art is carried out substantial improvements, a kind of preparation method's science, reasonable is provided, energy consumption is low, cost is low utilizes carbide slag to prepare the method for calcium polysilicate aluminium coagulating agent, and with the good stability of the calcium polysilicate aluminium coagulating agent of method for preparing, the treating water effect is good.
The objective of the invention is to realize by following technical scheme:
A kind of method of utilizing carbide slag to prepare polymeric silicicacid calcium aluminium coagulating agent is characterized in that it comprises following step:
(1) carbide slag is carried out drying treatment, 100 ℃～200 ℃ of carbide slag drying temperatures, time of drying 2～6h.Dried carbide slag is Powdered;
(2) carry out purification processes after the carbide slag drying treatment, the mass ratio of getting carbide slag that step (1) obtains and ammonification ammonium is 1～6, preparation water is 200～1200ml, 20 ℃～60 ℃ of controlled temperature, regulate pH=7～9, control stirring velocity 100～300r/min, churning time 20～30min leaves standstill 20～30min and obtains the carbide slag extracting solution;
(3) prepare silicon acid sodium solution, described sodium silicate solution percentage concentration is 4%～8%, with SiO
2The massfraction meter, the pH of the sodium silicate solution of the vitriol oil with 10%～30% or sodium hydroxide adjusting 4%～8% is 1～3, obtains poly-silicate solution;
(4) the poly-silicate solution that step (3) is obtained carries out polycondensation, and the reaction times is 0.5～1.5h, obtains high poly-silicate solution, this solution emulsus emulsus liquid state that is white in color;
(5) alum liquor concentration is 0.03～0.1mol/L, and the mol ratio of Al and Si is 0.3～0.8, and the mol ratio of Ca and Si is 0.2～0.8;
(6) under room temperature, stirring velocity 50～150r/min, churning time 1～5min condition, in the poly-silicate solution of height, add the alum liquor 100mL that step (5) is obtained;
(7) under room temperature, stirring velocity 50～150r/min, the churning time 1～5min condition, in poly-silicic acid of the height that step (6) obtains and Tai-Ace S 150 mixing solutions, add the carbide slag extracting solution 100mL that step (2) obtains, the heavyization time is 4～10h, it is 14.1%～15.6% polymeric silicicacid calcium aluminium coagulating agent product that preparation becomes massfraction, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
It is simple that preparation of the present invention has a processing step, the characteristics of low cost of manufacture.Reaction is carried out at normal temperatures, is easy to control, good stability.Flocculate rapidly when product is used as flocculation agent, flco is big and solid, and sedimentation is fast, applied range, suitable pH wide ranges.Preparation method of the present invention is easy to realize that can realize suitability for industrialized production calcium polysilicate aluminium, product has broad application prospects at water treatment field, and economic benefit is considerable.
Embodiment
Embodiment 1: the power taking rock ballast carries out drying treatment, 100 ℃ of carbide slag kiln temperatures, time of drying 2h, obtaining massfraction is 40.5% Powdered carbide slag; Use ammonium chloride during purification, the mass ratio of carbide slag and ammonification ammonium is 1, power taking rock ballast 3.6g, ammonium chloride 3.6g, in 200mL preparation water, mix, control 20 ℃ of its temperature, pH=7, stirring velocity 100r/min, churning time 20min, leave standstill 20min, obtain the carbide slag extracting solution of calcium ions 0.02mol/L; Get 10ml, 4% sodium silicate solution is incorporated in 5ml, 10% sulphuric acid soln; The pH that utilizes 10% sodium hydroxide and sulfuric acid to regulate sodium silicate solution is 1, obtains poly-silicate solution; The control polycondensation reaction time is 0.5h, obtains the high poly-silicate solution of white emulsus; Introduce 0.03mol/L, the alum liquor calcium ions 0.02mol/L of 100mL, the carbide slag extracting solution of 100mL in the poly-silicate solution of height after polycondensation; Under room temperature, stirring velocity 50r/min, the churning time 1min condition, polycondensation takes place; The heavyization time is 4h, obtains 14.1% polymeric silicicacid calcium aluminium coagulating agent, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
Embodiment 2: the power taking rock ballast carries out drying treatment, 150 ℃ of carbide slag kiln temperatures, time of drying 4 h, obtaining massfraction is 43.6% Powdered carbide slag; Carbide slag carries out will carrying out purification processes after the drying treatment, uses ammonium chloride during purification; The mass ratio of carbide slag and ammonification ammonium is 3, power taking rock ballast 10.8g, ammonium chloride 3.6g mixes in 700mL preparation water, controls 40 ℃ of its temperature, pH=8, stirring velocity 200r/min, churning time 25min, leaves standstill the carbide slag extracting solution that 25min obtains calcium ions 0.05mol/L; Get 20ml, 6% sodium silicate solution, be incorporated in 7ml, 20% sulphuric acid soln under the control stirring velocity 100r/min condition; The pH that utilizes 20% sodium hydroxide and sulfuric acid to regulate sodium silicate solution is 2; The control polycondensation reaction time is 1.0h, obtains the high poly-silicate solution of white emulsus; Introduce 0.06mol/L successively in the poly-silicate solution of height after polycondensation, the alum liquor calcium ions 0.05mol/L of 100mL, polycondensation under room temperature, stirring velocity 100r/min, the churning time 3min condition, takes place in the carbide slag extracting solution of 100mL; The heavyization time is 8h, obtains 14.6% polymeric silicicacid calcium aluminium coagulating agent, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
Embodiment 3: the power taking rock ballast carries out drying treatment, 200 ℃ of carbide slag kiln temperatures, time of drying 6h, obtaining massfraction is 44.3% Powdered carbide slag; Carbide slag carries out will carrying out purification processes after the drying treatment, uses ammonium chloride during purification; The mass ratio of carbide slag and ammonification ammonium is 6, power taking rock ballast 21.6g, ammonium chloride 3.6g mixes in 1200mL preparation water, controls 60 ℃ of its temperature, pH=9, stirring velocity 300r/min, churning time 30min, leaves standstill the carbide slag extracting solution that 30min obtains calcium ions 0.08mol/L; Get 30ml, 8% sodium silicate solution, be incorporated in 10ml, 30% sulphuric acid soln under the control stirring velocity 150r/min condition; The pH that utilizes 30% sodium hydroxide and sulfuric acid to regulate sodium silicate solution is 3; The control polycondensation reaction time is 1.5h, obtains the high poly-silicate solution of white emulsus; Introduce 0.1mol/L successively in the poly-silicate solution of height after polycondensation, the alum liquor of 100mL and calcium ions 0.08mol/L, polycondensation under room temperature, stirring velocity 150r/min, the churning time 5min condition, takes place in the extracting solution of 100mL; The heavyization time is 10h.Obtain 15.6% polymeric silicicacid calcium aluminium coagulating agent, polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
Ammonium chloride, Tai-Ace S 150 adopt analytical pure, sodium hydroxide, and raw materials such as sulfuric acid are easy to get, and are the commercially available prod.
The related loft drier of the method for utilizing carbide slag to prepare polymeric silicicacid calcium aluminium coagulating agent of the present invention, agitator etc. are the commercially available prod.
Claims (1)
1. method of utilizing carbide slag to prepare polymeric silicicacid calcium aluminium coagulating agent is characterized in that it comprises following step:
(1) carbide slag is carried out drying treatment, 100 ℃～200 ℃ of carbide slag drying temperatures, time of drying 2～6h.Dried carbide slag is Powdered;
(2) carry out purification processes after the carbide slag drying treatment, the mass ratio of getting carbide slag that step (1) obtains and ammonification ammonium is 1～6, preparation water is 200～1200ml, 20 ℃～60 ℃ of controlled temperature, regulate pH=7～9, control stirring velocity 100～300r/min, churning time 20～30min leaves standstill 20～30min and obtains the carbide slag extracting solution;
(3) prepare silicon acid sodium solution, described sodium silicate solution percentage concentration is 4%～8%, with SiO
2The massfraction meter, the pH of the sodium silicate solution of the vitriol oil with 10%～30% or sodium hydroxide adjusting 4%～8% is 1～3, obtains poly-silicate solution;
(4) the poly-silicate solution that step (3) is obtained carries out polycondensation, and the reaction times is 0.5～1.5h, obtains high poly-silicate solution, this solution emulsus emulsus liquid state that is white in color;
(5) alum liquor concentration is 0.03～0.1mol/L, and the mol ratio of Al and Si is 0.3～0.8, and the mol ratio of Ca and Si is 0.2～0.8;
(6) under room temperature, stirring velocity 50～150r/min, churning time 1～5min condition, in the poly-silicate solution of height, add the alum liquor 100mL that step (5) is obtained;
(7) under room temperature, stirring velocity 50～150r/min, the churning time 1～5min condition, in poly-silicic acid of the height that step (6) obtains and Tai-Ace S 150 mixing solutions, add the carbide slag extracting solution 100mL that step (2) obtains, the heavyization time is 4～10h, it is 14.1%～15.6% polymeric silicicacid calcium aluminium coagulating agent product that preparation becomes massfraction, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821413A (en) * | 2018-07-10 | 2018-11-16 | 无锡锐众环保科技有限公司 | A kind of coagulant of efficient process COD |
| CN115368164A (en) * | 2022-08-31 | 2022-11-22 | 山东鲁碧绿色建筑科技有限公司 | Preparation method of porous concrete for external wall panel |
Citations (4)
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| CN1059505A (en) * | 1991-09-28 | 1992-03-18 | 张伯温 | Polymeric silicicacid-aluminium composite flocculation agent and preparation method |
| WO2001034294A1 (en) * | 1999-11-12 | 2001-05-17 | University Of Greenwich | Silicate/aluminate materials |
| CN101823721A (en) * | 2010-03-19 | 2010-09-08 | 合肥学院 | Method for producing poly silicate aluminium ferric flocculating agent by utilizing coal gangue |
| CN101830476A (en) * | 2009-03-13 | 2010-09-15 | 抚顺矿业集团有限责任公司 | Method for preparing polymeric ferric aluminum silicate flocculant from waste oil shale slag |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059505A (en) * | 1991-09-28 | 1992-03-18 | 张伯温 | Polymeric silicicacid-aluminium composite flocculation agent and preparation method |
| WO2001034294A1 (en) * | 1999-11-12 | 2001-05-17 | University Of Greenwich | Silicate/aluminate materials |
| CN101830476A (en) * | 2009-03-13 | 2010-09-15 | 抚顺矿业集团有限责任公司 | Method for preparing polymeric ferric aluminum silicate flocculant from waste oil shale slag |
| CN101823721A (en) * | 2010-03-19 | 2010-09-08 | 合肥学院 | Method for producing poly silicate aluminium ferric flocculating agent by utilizing coal gangue |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821413A (en) * | 2018-07-10 | 2018-11-16 | 无锡锐众环保科技有限公司 | A kind of coagulant of efficient process COD |
| CN115368164A (en) * | 2022-08-31 | 2022-11-22 | 山东鲁碧绿色建筑科技有限公司 | Preparation method of porous concrete for external wall panel |
| CN115368164B (en) * | 2022-08-31 | 2023-06-06 | 山东鲁碧绿色建筑科技有限公司 | Preparation method of porous concrete for external wall panel |
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